CN102764895B - Device and method for preparing high-purity ultrafine nickel powder - Google Patents
Device and method for preparing high-purity ultrafine nickel powder Download PDFInfo
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- CN102764895B CN102764895B CN201210268925.5A CN201210268925A CN102764895B CN 102764895 B CN102764895 B CN 102764895B CN 201210268925 A CN201210268925 A CN 201210268925A CN 102764895 B CN102764895 B CN 102764895B
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Abstract
The invention provides a reaction device for preparing ultrafine metal powder and a method for preparing high-purity ultrafine nickel powder. Four small quartz inner tubes are arranged in one large quartz outer tube. A horizontal tube furnace is sleeved outside the outer tube and used for controlling the chemical reaction temperature in the outer tube. A coarse metal powder (or metal oxide) is put in a quartz boat of the third inner tube and chloridized into a metal chloride by high-temperature chlorine or chlorine and carbon monoxide, the latter one volatiles at high temperature and is blown into the fourth inner tube by argon to subject to gas-gas reduction reaction with hydrogen blown into the first inner tube to generate vapor-phase nickel powder, and the vapor-phase nickel powder is mainly taken away from a high-temperature area by the high-speed argon blown into the second inner tube and taken into a low-temperature area and adhered to the low-temperature inner wall of the fourth inner tube, thus the of the grow of the nickel powder through high-temperature sintering can be avoided. When the coarse nickel is chloridized, if no inorganic solid chloride is added, 82% of nickel is chloridized, and if sodium chloride was is added, 97% of nickel is chloridized.
Description
technical field
The present invention relates to a kind of reaction unit and method of preparing super-fine metal powder, more specifically relate to a kind of apparatus and method of preparing high-purity superfine metal simple substance nickel powder.
Background technology
Conventionally the powder body material that particle diameter is less than to 1 μ m calls superfine powdery material.Super-fine metal powder, because of its special character, has a wide range of applications.For example extra-fine nickel powder is a kind of rocket combustion adjuvant, adds it can make rocket burn rate improve 100 times.Extra-fine nickel powder is a kind of as submicron particle, because it has great skin effect and bulk effect, the physicochemical properties that demonstrate a series of uniquenesses at aspects such as magnetic, thermal resistance, interior pressure, light absorption, chemisms, all have broad application prospects in many fields such as magnetic material, catalyst, battery material, coating material, hardmetall binders.Due to technical reason, at present, China also cannot make extra-fine nickel powder, needs a large amount of imports.
At present, it is several that the method for preparing nickel powder both at home and abroad mainly contains hydroxyl nickel thermal decomposition method and liquid phase reduction etc.It is more that liquid phase reduction is prepared nickel powder research, but the nickel powder of preparation often contains moisture thus, and the latter can be oxidized the nickel simple substance of tool strong reducing property, and making it can not stable existence, thereby is in fact difficult to make nickel simple substance by liquid phase reduction.
From calculation of thermodynamics, can make elemental metals nickel, i.e. NiCl with hydrogen reducing Dehydrated nickel chloride
2+ H
2=Ni+2HCl.But nickel chloride (NiCl
2) very easily water suction, thereby commercial cannot buying, can not be as the raw material of preparing elemental metals nickel.Therefore, need to be that raw material is prepared Dehydrated nickel chloride through dry chloridising by cheap nickel powder (being called for short thick nickel powder) or similar dry oxidation nickel (NiO) powder that particle diameter is large, purity is not high, then prepare thus ultra-fine elemental metals nickel powder.But there are two difficult problems here, the one, how thick nickel powder or dry oxidation nickel are converted into Dehydrated nickel chloride as much as possible; The 2nd, how by Dehydrated nickel chloride, to make extra-fine nickel powder.
Summary of the invention
in order to address the above problem,the present invention proposes a kind of device and method of preparing high pure and ultra-fine nickel powder, and this device not only can be used for preparing high pure and ultra-fine nickel powder, also can be used for preparing the superfine powder of some other metal.
The present invention has mainly proposed a kind of crude metal nickel powder (or thick dry oxidation nickel) Efficient Conversion is Dehydrated nickel chloride, then Dehydrated nickel chloride in-situ reducing is become to the apparatus and method of high pure and ultra-fine nickel powder.Here " slightly " one refers to that raw material particle size is much larger than 1 micron, and two refer to that material purity is not high, greatly about 95-99%.This device not only can be used for preparing extra-fine nickel powder, also can be used for preparing the superfine powder of some other metal.These metals comprise elemental silicon, iron, cobalt, platinum group metal, gold, germanium, molybdenum, tungsten etc.
Technical scheme of the present invention is: a kind of device of preparing high-purity superfine metal nickel powder, this device comprises source of the gas, gas drying tube, gas mass flow controller, seal nipple, the first reaction tube, the second reaction tube, the 3rd reaction tube, the 4th reaction tube, outer tube, tube furnace, conduit, absorption plant and exhaust gas processing device.
One end mouth of pipe of described the 4th reaction tube is large diameter horn-like;
Described tube furnace is upper lower open-type horizontal pipe stove;
Wherein, described outer tube two ends are sealed and are placed in described tube furnace by seal nipple, the large diameter horn-like nose end of described the 4th reaction tube is inserted into described outer tube from outlet side, one end of described the first reaction tube and three reaction tubes is in inlet end is inserted into the horn-like mouth of pipe of described the 4th reaction tube described outer tube, described the second reaction tube is inserted into described outer tube from inlet end, described source of the gas is connected with one end of described gas mass flow controller by described gas drying tube, the other end of described gas mass flow controller by described seal nipple respectively with described the first reaction tube, the second reaction tube, the other end of the 3rd reaction tube connects, described absorption plant is connected with the other end of described the 4th reaction tube with seal nipple by conduit, described exhaust gas processing device is connected with described absorption plant by conduit.
Further, described the first reaction tube, the second reaction tube, the 3rd reaction tube, the 4th reaction tube and outer tube all adopt quartz to make.
Another object of the present invention is to provide the technique that said apparatus is prepared superfine metal elemental nickel, specifically comprises the following steps:
Step 1: be that micron inoganic solids chloride that the raw material crude metal elemental nickel of 1-300 micron or the oxide of thick nickel are 1-300 with particle diameter be take the ratio that the ratio of molal quantity is 1:1-10 and mixed by particle diameter, be contained in quartz boat, described quartz boat is placed in to the position of the end of keeping right of the 3rd reaction tube, the 100 mL/min flows of at room temperature take pass into concentration as more than 99.99% inert gas in the 3rd reaction tube, keep 0.2-1h, under logical inert gas, start diamond heating, while being heated to 650-1000 ℃, stop logical inert gas, change to pass into and take chlorine or chlorine and the carbon monoxide that flow is 200 mL/min, react after 0.5-6 hour, stop logical chlorine, with 50 mL/min flows, pass into inert gas, obtain solid water-free nickel chloride, wherein, the mass ratio of described chlorine and carbon monoxide is 1:0.2-30, described inoganic solids chloride is sodium chloride, potassium chloride, calcium chloride or magnesium chloride, ferric trichloride or ferrous chloride,
Step 2: start described diamond heating under the atmosphere of inert gas, when being heated to the temperature of 700-1000 ℃, make Dehydrated nickel chloride volatilization, respectively to blown inert gas in the second reaction tube and the 3rd reaction tube, in the first reaction tube, be blown into hydrogen, the Dehydrated nickel chloride of volatilization is blown out the 3rd reaction tube by inert gas and enters the hydrogen blowing out with the first reaction tube in the 4th reaction tube and in the 4th reaction tube, meet and react and generate gas phase nickel powder, meanwhile, the second reaction tube blows out inert gas further to be accelerated gas phase nickel powder and mist in the 4th reaction tube, by horn mouth high-temperature region, to be transferred to tubule mouth low-temperature space cooling, be adsorbed on the tube wall of the 4th reaction tube low-temperature space, be not cooled gas phase nickel powder and mist enters into absorption plant by conduit and exhaust gas processing device is processed of part, wherein, the ratio of the gas flow passing into of the first reaction tube, the second reaction tube and the 3rd reaction tube is 1:2-20:2-20,
Step 3: at room temperature remove with absolute ethanol washing the nickel powder being bonded on the 4th reaction tube 10 inwalls, nickel powder sinks to solution bottom, with magnet, hold solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by chloride solution, repeatedly use absolute ethanol washing nickel powder; The treating apparatus processing that also uses the same method, obtains purifying nickel powder.
Further, described inert gas is argon gas, helium or nitrogen.
What further, in described step 2, absorption plant was processed the gas phase nickel powder volatilize on a small quantity is absolute ethyl alcohol; What described exhaust gas processing device was processed mist is that concentration is the sodium hydroxide solution of 5-20%.
The principle of the inventive method is: by thick nickel powder (or dry oxidation nickel) and inoganic solids chloride as sodium chloride or/and the powder such as potassium chloride are put into the quartz boat of the 3rd reaction tube after fully mixing, then in the 3rd reaction tube, lead to drying chlorine (or drying chlorine adds carbon monoxide), about 700 ℃ reactions, generate Dehydrated nickel chloride, the Dehydrated nickel chloride generating as sodium chloride and reaction due to inoganic solids chloride forms eutectic compound (2NaClNiCl
2), i.e. Ni+Cl
2+ 2NaCl=2NaClNiCl
2, or NiO+Cl
2+ 2NaCl+CO=2NaClNiCl
2+ CO
2, this reduces the dry chlorination Gibbs free energy of thick nickel powder (or dry oxidation nickel), and thick nickel powder (or dry oxidation nickel) chlorination conversion ratio improves.The application's research shows, during the chlorination of crude metal nickel, does not add inoganic solids chloride, and the chlorination rate of nickel is 82%; Add sodium chloride, the chlorination rate of nickel is brought up to 97% left and right.Eutectic compound (2NaClNiCl
2) fusing point is compared with NiCl
2or NaCl is low.Anhydrous NiCl
2fusing point is 1001 ℃, the anhydrous NiCl that dry chlorination obtains
2in higher temperatures (700-1000 ℃), can volatilize, the inert gas for Dehydrated nickel chloride of volatilization is (as Ar or N
2deng) blow out the 3rd reaction tube and enter in the 4th reaction tube, the hydrogen blowing out in this and first reaction tube meets, and generates gas phase nickel powder, i.e. NiCl and react
2+ H
2=Ni+2HCl.Meanwhile, second reaction tube can blow out inert gas (as Ar or N
2deng).The mixed airflow that gas phase nickel powder is blown out by first, second and third reaction tube is bonded on the low temperature wall of the 4th reaction tube with entered low-temperature space condensation by high-temperature region.Due to anhydrous NiCl in inert gas
2and H
2concentration is all very low, strafes electric Microscopic observation and finds, both react and generate the very little regular cube type superfine metal nickel simple substance of particle diameter.Add inert gas flow speed very fast, it takes away rapidly high temperature reaction zone by above-mentioned superfine metal nickel and enters low-temperature space, grows up, so obtained extra-fine nickel powder so above-mentioned superfine metal nickel has little time sintering.Because chlorination temperature (700 ℃ of left and right) is not high, MgO, Cr in thick nickel powder
2o
3not high Deng chlorination degree.Owing to only having, metal chloride volatility is larger, and metal oxide volatility is much lower compared with chloride.During high temperature (700-1100 ℃) reduction, under inert gas (as argon gas or nitrogen) blows, be mainly anhydrous NiCl
2enter gas phase, and there is no MgO, the Cr of chlorination
2o
3, can not volatilize, thereby volatilization enters the anhydrous NiCl of gas phase
2purity is higher.In addition, even a small amount of MgO, Cr
2o
3formed corresponding chloride, these chlorides can not be become metal simple-substance by hydrogen reducing, when with absolute ethanol washing extra-fine nickel powder mixture, these metal chlorides or be dissolved in absolute ethyl alcohol or swim in ethanol solution top, with magnet, hold container bottom nickel powder, by decant method repeatedly, will swim in ethanol solution top common salt solid separated with nickel powder, thereby the extra-fine nickel powder purity obtaining is very high.
Particularly, the present invention proposes a kind of tube furnace reaction unit that raw material crude metal powder (or thick anhydrous metal oxide) is converted into high-purity superfine metal powder.Here " slightly " one refers to that raw material particle size is much larger than 1um, and two refer to that material purity is not high, greatly about 95-99%.Said apparatus comprises:
The present invention compared with prior art, has the following advantages and beneficial effect:
The method all processes anhydrous and without high temperature (higher than room temperature) air conditions under carry out, the extra-fine nickel powder obtaining almost not and water or air react;
2. the Dehydrated nickel chloride making in the method is without taking out reactor, but by the volatilization of its in-situ high temperature, use inert gas is (as Ar or N
2deng) Dehydrated nickel chloride of volatilization is blown in gas phase and hydrogen generation gas-solid/liquid/gas reactions, thereby the preparation of Dehydrated nickel chloride and Dehydrated nickel chloride hydrogen reduction are subsequently carried out continuously in same reactor.Reaction unit is simple, and method saves time.
Accompanying drawing explanation
Fig. 1 is the overall structure schematic diagram of reaction unit of the present invention.
Fig. 2 is local enlarged diagram of the present invention.
In figure:
1. source of the gas, 2. gas drying tube, 3. gas mass flow controller, 4. seal nipple, 5. the first reaction tube, 6. the second reaction tube, 7. the 3rd reaction tube, 8. quartz boat, 9. tube furnace, 10. the 4th reaction tube, 11. outer tubes, 12.L type conduit, 13. absorption plants, 14. exhaust gas processing devices.
The specific embodiment
Below in conjunction with concrete drawings and Examples, technical scheme of the present invention is described further.
For the present invention, prepare as illustrated in fig. 1 and 2 the device schematic diagram of high-purity superfine metal nickel powder, this device comprises source of the gas 1, gas drying tube 2, gas mass flow controller 3, seal nipple 4, the first reaction tube 5, the second reaction tube 6, the 3rd reaction tube 7, quartz boat 8, tube furnace 9, the 4th reaction tube 10, outer tube 11, L-type conduit 12, absorption plant 13 and exhaust gas processing device 14.
Wherein, one end mouth of pipe of the 4th reaction tube 10 is large diameter horn-like;
Tube furnace 9 is upper lower open-type horizontal pipe stove;
The two ends of outer tube 11 seal by seal nipple 4, and outer tube 11 is placed in tube furnace 9, the opening that is of the 4th reaction tube 10 is trumpet-shaped one end and is inserted into outer tube 11 from outlet side, one end of the first reaction tube 5 and the 3rd reaction tube 7 from inlet end be inserted into the 4th reaction tube 10 outer tube 11 be opening be horn-like in, one end of the second reaction tube 6 is inserted into outer tube 11 from inlet end, source of the gas 1 is connected with gas mass flow controller 3 by gas drying tube 2, gas mass flow controller 3 by seal nipple 4 respectively with the first reaction tube 5, the second reaction tube 6 and the 3rd reaction tube 7 other ends are tightly connected, absorption plant 13 is tightly connected by conduit 12 and seal nipple 4 and the 4th reaction tube 10, exhaust gas processing device 14 is connected with absorption plant 13 by conduit 12.
By the particle diameter 0.050-0.057 millimeter thick nickel powder of 1.0 g and with particle diameter 0.050-0.100 millimeter 1.62 g MgCl
2dried powder mixes in the quartz boat 8 shown in load map 1.At room temperature in the 3rd reaction tube 7, lead to 100 mL/min high-purity argon gas 30 minutes.Under the logical argon gas condition of the 3rd reaction tube 7, tube furnace 9 is warming up to 900 ℃, then 100 mL/min argon gas are switched to 200 mL/min chlorine reaction 2 hours.Then 200 mL/min chlorine are switched to 50 mL/min argon gas.Obtain solid water-free nickel chloride, tube furnace 9 temperature are risen to 750 ℃, in the second reaction tube 6, lead to 150 mL/min argon gas simultaneously, in the first reaction tube 5, lead to 50 mL/min hydrogen, in the 3rd reaction tube 7, lead to 150 mL/min argon gas.Above argon gas and hydrogen purity are 99.99% above high-purity gas, tube furnace 9 is lowered the temperature naturally, all Dehydrated nickel chlorides are all evaporated completely in quartz boat 8 after measured afterwards, at room temperature with absolute ethanol washing, remove the nickel powder being bonded on reaction tube 10 inwalls, the magnesium chloride mixture solution that obtains being insoluble to the nickel powder of absolute ethyl alcohol and be dissolved in absolute ethyl alcohol.After solution left standstill, magnesium chloride is dissolved in ethanol solution, and nickel powder sinks to solution bottom, with magnet, hold solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by magnesium chloride solution, repeatedly use absolute ethanol washing nickel powder, obtain purifying nickel powder, it is kept in absolute ethyl alcohol.Through x ray fluorescence (XRF) and transmission electron microscope (TEM) mensuration, find not contain any impurity in nickel powder, with strafing the nickel particle that electron microscope (SEM) observes, be regular regular cube, the length of side overwhelming majority is less than 0.1 micron, and what therefore obtain is high pure and ultra-fine nickel powder.
By the particle diameter 0.050-0.057 millimeter thick nickel oxide powder of 1.0 g with particle diameter 0.050-0.100 millimeter 1.99 g NaCl dried powders, mix in the quartz boat 8 shown in load map 1.At room temperature in the 3rd reaction tube 7, lead to 100 mL/min high-purity argon gas 1h.Under the logical argon gas condition of the 3rd reaction tube 7, tube furnace 9 is warming up to 1000 ℃, then 100 mL/min argon gas are switched to 200 mL/min(with mass ratio 1:30, mixes) chlorine and reaction of carbon monoxide 3.5 hours.Then 200 mL/min chlorine are switched to 50 mL/min argon gas, logical argon gas 3h.
Then under logical 50 mL/min argon gas conditions, tube furnace 9 heating are risen to 950 ℃.And then in the second reaction tube 6, lead to 150 mL/min argon gas, in the first reaction tube 5, lead to 50 mL/min hydrogen, in the 3rd reaction tube 7, lead to 150 mL/min argon gas.Above argon gas and hydrogen purity are 99.99% above high-purity gas, tube furnace 9 is lowered the temperature naturally, all Dehydrated nickel chlorides are all evaporated completely in quartz boat 8 after measured afterwards, at room temperature with absolute ethanol washing, remove the nickel powder being bonded on the 4th reaction tube 10 inwalls, obtain being insoluble to nickel powder and the common salt solid mixture solution of absolute ethyl alcohol.After solution left standstill, common salt solid floats over ethanol solution top, and nickel powder sinks to solution bottom, with magnet, hold solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by common salt solid, repeatedly use absolute ethanol washing nickel powder, obtain nickel powder, it is kept in absolute ethyl alcohol.Through x ray fluorescence (XRF) and transmission electron microscope (TEM) mensuration, find not contain any impurity in nickel powder, with strafing the nickel particle that electron microscope (SEM) observes, be regular regular cube, the length of side overwhelming majority is less than 0.1 micron, and what therefore obtain is high pure and ultra-fine nickel powder.
By the particle diameter 0.050-0.057 millimeter thick nickel powder of 1.0 g and with particle diameter 0.050-0.100 millimeter 1.98g CaCl
2dried powder mixes in the quartz boat 8 shown in load map 1.At room temperature in the 3rd reaction tube 7, lead to 100 mL/min high-purity argon gas 0.2h.Under the logical argon gas condition of the 3rd reaction tube 7, tube furnace 9 is warming up to 850 ℃, then 100 mL/min argon gas are switched to 200 mL/min chlorine reaction 6 hours.Then 200 mL/min chlorine are switched to 50 mL/min argon gas, logical argon gas 6h, obtains anhydrous chlorides of rase and receives solid;
Then under logical 50 mL/min argon gas conditions, tube furnace 9 is heated to 900 ℃.And then in the second reaction tube 6, lead to 150 mL/min argon gas, in the first reaction tube 5, lead to 50 mL/min hydrogen, in the 3rd reaction tube 7, lead to 150 mL/min argon gas.Above argon gas and hydrogen purity are 99.99% above high-purity gas, tube furnace 9 is lowered the temperature naturally, all Dehydrated nickel chlorides are all evaporated completely in quartz boat 8 after measured afterwards, at room temperature with absolute ethanol washing, remove the nickel powder being bonded on the 4th reaction tube 10 inwalls, the calcium chloride mixture solution that obtains being insoluble to the nickel powder of absolute ethyl alcohol and be dissolved in absolute ethyl alcohol.After solution left standstill, calcium chloride is dissolved in ethanol solution, and nickel powder sinks to solution bottom, with magnet, hold solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by magnesium chloride solution, repeatedly use absolute ethanol washing nickel powder, obtain purifying nickel powder, it is kept in absolute ethyl alcohol.Through x ray fluorescence (XRF) and transmission electron microscope (TEM) mensuration, find not contain any impurity in nickel powder, with strafing the nickel particle that electron microscope (SEM) observes, be regular regular cube, the length of side overwhelming majority is less than 0.1 micron, and what therefore obtain is high pure and ultra-fine nickel powder.
By the particle diameter 0.050-0.057 millimeter thick nickel oxide powder of 1.0 g with particle diameter 0.050-0.100 millimeter 2.54g KCl dried powder, mix in the quartz boat 8 shown in load map 1.At room temperature in the 3rd reaction tube 7, lead to 100 mL/min high-purity argon gas 0.5 hour.Under the logical argon gas condition of the 3rd reaction tube 7, tube furnace 9 is warming up to 1000 ℃, then 100 mL/min argon gas are switched to 200 mL/min(with mass ratio 1:1, mixes) chlorine and reaction of carbon monoxide 4 hours.Then 200 mL/min chlorine are switched to 50 mL/min argon gas, logical argon gas 6h, obtains Dehydrated nickel chloride solid;
Then under logical 50 mL/min argon gas conditions, tube furnace 9 is heated to 700 ℃.And then in the second reaction tube 6, lead to 150 mL/min argon gas, in the first reaction tube 5, lead to 50 mL/min hydrogen, in the 3rd reaction tube 7, lead to 150 mL/min argon gas.Above argon gas and hydrogen purity are 99.99% above high-purity gas, tube furnace 9 is lowered the temperature naturally, all Dehydrated nickel chlorides are all evaporated completely in quartz boat 8 after measured afterwards, at room temperature with absolute ethanol washing, remove the nickel powder being bonded on the 4th reaction tube 10 inwalls, obtain being insoluble to nickel powder and the solid potassium chloride mixture solution of absolute ethyl alcohol.After solution left standstill, solid potassium chloride floats over ethanol solution top, and nickel powder sinks to solution bottom, with magnet, holds solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by solid potassium chloride, obtains nickel powder, and it is kept in absolute ethyl alcohol.Through x ray fluorescence (XRF) and transmission electron microscope (TEM) mensuration, find not contain any impurity in nickel powder, with strafing the nickel particle that electron microscope (SEM) observes, be regular regular cube, the length of side overwhelming majority is less than 0.1 micron, and what therefore obtain is high pure and ultra-fine nickel powder.
Claims (3)
1. a method of preparing high pure and ultra-fine nickel powder, its preparation facilities comprises source of the gas (1), gas drying tube (2), gas mass flow controller (3), seal nipple (4), the first reaction tube (5), the second reaction tube (6), the 3rd reaction tube (7), the 4th reaction tube (10), outer tube (11), tube furnace (9), L shaped conduit (12), absorption plant (13) and exhaust gas processing device (14);
One end mouth of pipe of described the 4th reaction tube (10) is large diameter horn-like;
Described tube furnace (9) is upper lower open-type horizontal pipe stove;
Wherein, described outer tube (11) two ends are by seal nipple (4) sealing, and described outer tube (11) is placed in described tube furnace (9); The large diameter horn-like nose end of described the 4th reaction tube (10) is inserted into described outer tube (11) inside from outlet side, one end of described the first reaction tube (5) and the 3rd reaction tube (7) is inserted in the horn-like mouth of pipe of described the 4th reaction tube (10) in described outer tube (11) from inlet end, described the second reaction tube (6) is inserted into described outer tube (11) inside from inlet end
Described source of the gas (1) is connected with described gas mass flow controller (3) by described gas drying tube (2), described gas mass flow controller (3) is connected with the other end of described the first reaction tube (5), the second reaction tube (6), the 3rd reaction tube (7) respectively by described seal nipple (4), described absorption plant is tightly connected with the other end of described the 4th reaction tube (10) by L-type conduit (12) and seal nipple (4), and described exhaust gas processing device (14) is connected with described absorption plant (13) by L-type conduit (12); The first reaction tube (5), the second reaction tube (6), the 3rd reaction tube (7), the 4th reaction tube (10) and outer tube (10) all adopt quartz to make, and specifically comprise the following steps:
Step 1: be that micron inoganic solids chloride that the raw material crude metal elemental nickel of 1-300 micron or the oxide of thick nickel are 1-300 with particle diameter be take the ratio that the ratio of molal quantity is 1:1-10 and mixed by particle diameter, be contained in quartz boat, described quartz boat is placed in to the position of the end of keeping right of the 3rd reaction tube, the 100 mL/min flows of at room temperature take pass into concentration as more than 99.99% inert gas in the 3rd reaction tube, keep 0.2-1h, under logical inert gas, start diamond heating again, while being heated to 650-1000 ℃, stop logical inert gas, change to pass into and take chlorine or chlorine and the carbon monoxide that flow is 200 mL/min, react after 0.5-6 hour, stop logical chlorine or chlorine and carbon monoxide, with 50 mL/min flows, pass into inert gas, obtain solid water-free nickel chloride, wherein, the mass ratio of described chlorine and carbon monoxide is 1:0.2-30, and described inoganic solids chloride is sodium chloride, potassium chloride, calcium chloride, magnesium chloride, ferric trichloride or ferrous chloride,
Step 2: respectively to blown inert gas in the second reaction tube and the 3rd reaction tube, in the first reaction tube, be blown into hydrogen, the Dehydrated nickel chloride of volatilization is blown out the 3rd reaction tube by inert gas and enters the hydrogen blowing out with the first reaction tube in the 4th reaction tube and in the 4th reaction tube, meet and react and generate gas phase nickel powder, meanwhile, the second reaction tube blows out inert gas further to be accelerated gas phase nickel powder and mist in the 4th reaction tube, by horn mouth high-temperature region, to be transferred to tubule mouth low-temperature space cooling, obtain on tube wall that high pure and ultra-fine nickel powder is adsorbed on the 4th reaction tube low-temperature space, the gas phase composition and the mist that are not adsorbed enter into absorption plant and exhaust gas processing device by conduit, wherein, the ratio of the gas flow passing into of the first reaction tube, the second reaction tube and the 3rd reaction tube is 1:2-20:2-20,
Step 3: at room temperature remove with absolute ethanol washing the nickel powder being bonded on the 4th reaction tube (10) inwall, nickel powder sinks to solution bottom, with magnet, hold solution bottom nickel powder, with repeatedly decant method is separated with nickel powder by chloride solution, repeatedly use absolute ethanol washing nickel powder; The treating apparatus processing that also uses the same method, obtains purifying nickel powder.
2. method according to claim 1, is characterized in that, described inert gas is argon gas or helium.
3. method according to claim 1, is characterized in that, what in described step 2, absorption plant was processed the gas phase nickel powder volatilize on a small quantity is absolute ethyl alcohol; What described exhaust gas processing device was processed mist is that concentration is the sodium hydroxide solution of 5-20%.
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| CN103498059B (en) * | 2013-09-04 | 2015-04-22 | 昆明理工大学 | Method for making high-purity nickel by chlorination of electrolytic nickel |
| CN105043102B (en) * | 2015-04-16 | 2017-02-22 | 重庆大学 | Novel method for reducing sinter using hydrogen |
| CN107116228B (en) * | 2017-06-20 | 2019-01-04 | 中南大学 | A kind of method that solid phase reduction prepares extra-fine nickel powder |
| CN109269302A (en) * | 2018-11-09 | 2019-01-25 | 济南大学 | A kind of calcining vessel and method for calcinating |
| CN109336166A (en) * | 2018-11-21 | 2019-02-15 | 上海谦懋纺织科技有限公司 | A kind of manufacturing device and manufacturing method of efficient deodorizing porous zinc bloom nanometer cylinder |
| CN112974822B (en) * | 2021-02-08 | 2021-12-10 | 天津大学 | Preparation method of cotton-shaped metal nickel powder |
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| CN202254801U (en) * | 2011-07-13 | 2012-05-30 | 沈少波 | Tubular reaction furnace and chlorination reaction device with same |
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